CN104529165A - Yellow afterglow microcrystalline glass for AC-LED and preparation technology thereof - Google Patents

Yellow afterglow microcrystalline glass for AC-LED and preparation technology thereof Download PDF

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CN104529165A
CN104529165A CN201410738480.1A CN201410738480A CN104529165A CN 104529165 A CN104529165 A CN 104529165A CN 201410738480 A CN201410738480 A CN 201410738480A CN 104529165 A CN104529165 A CN 104529165A
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devitrified glass
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CN104529165B (en
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林航
王元生
徐桔
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Fujian Institute of Research on the Structure of Matter of CAS
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0054—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing PbO, SnO2, B2O3
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Ceramic Engineering (AREA)
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Abstract

The invention puts forward a Ln3Al2Ga3O12:Ce, R (Ln is one of Y, Gd and Lu; and R is one of Cr, Bi) microcrystalline glass able to realize efficient blue light excitation and yellow light afterglow emission and a preparation method thereof. According to the microcrystalline glass, Ln3Al2Ga3O12:Ce, R fluorescent microcrystallines are evenly inlaid in an oxide glass matrix. The microcrystalline glass emits yellow light under blue light excitation, and when excitation stops, bright yellow light afterglow emission can be realized. Under alternating current drive, an AC-LED prototype device constructed based on microcrystalline glass has a stroboscopic depth of only 49.5%. Thus, the microcrystalline glass can be developed and applied to novel high power remote white light AC-LED.

Description

A kind of yellow twilight sunset devitrified glass for AC-LED and technology of preparing thereof
Technical field
The present invention relates to solid luminescent material field, especially relate to yellow twilight sunset devitrified glass and preparation technology thereof that one can be applied to interchange (AC) LED.
Technical background
Current, on market, large power white light LED illuminating product needs to utilize AC/DC changeover switch civil power to be converted to direct current with driving LED load mostly.Be easy to because AC/DC changeover switch has electrolytic condenser in electric energy loss high (15-30%), device shortcomings such as damaging (life-span is generally lower than 10,000 hours), price is high, volume is large, constrain the system efficiency of LED component, actual service life, cost and appearance design to a great extent.Obviously, if can with the direct driving LED of alternating-current (AC-LED), just can solve the problem preferably, related products has the incomparable advantage of traditional DC-LED in multiple fields such as residential lighting, street lamp, office lighting, Landscape Lightings, is expected to the development trend leading large power white light LED illumination market new.
But the voltage change in sinusoidal function rule in time of alternating-current, only can light LED when inputting effective voltage value and exceeding forward voltage, this makes AC-LED occur the stroboscopic phenomenon that light and shade constantly converts in the loop cycle of alternating-current.Electric light source stroboscopic can visually produce serious negative effect people, is the large bottleneck that development AC-LED technology faces.Recently, Taiwan Univ. professor Liu Ruxi proposes to utilize the power-off persistence characteristic with specific life-span fluorescent material to reduce stroboscopic (Opt.Express, 2012,20,18031).Chinese patent CN 101705095 discloses a kind of aY towards AC-LED application 2o 3bAl 2o 3siO 2: the yellow persistence phosphor of mCenBxNayP, describes the stroboscopic that its afterglow (twilight sunset life-span: 5-20ms) successfully reduces AC-LED device.Chinese patent CN 102468413 discloses the multiple AC-LED lamp polychrome persistence phosphor being suitable for UV/blue chip and exciting.In view of AC-LED has wide market outlook, the AC-LED twilight sunset fluorescent material tool of Development of Novel is of great significance.
As everyone knows, the encapsulation of traditional LED product is mixed in by fluorescent material in organic polymer (epoxy resin or silica gel), is then directly coated in chip surface.Organic polymer material heat resistanceheat resistant and the radiation resistance of this technology existence encapsulation are poor, easily yellow occur, thus the serious difficult problem reducing great power LED work-ing life.Devitrified glass is the matrix material evenly having inlayed micro-/ nano crystalline substance in unorganic glass matrix, has that technology of preparing is simple, thermostability and a high advantage of chemical stability.Compared with organic packaging materials, its thermal conductivity is also much bigger.In addition, devitrified glass can be processed into tabular or bulb-shaped easily, and encapsulates away from chip.Therefore, if AC-LED lamp twilight sunset fluorescent microcrystalline can be separated out and form twilight sunset devitrified glass fluor and assemble long-range AC-LED in glass matrix, this new device by have simultaneously stroboscopic low, photochromic stable, luminescent quality is high, the remarkable advantage of long service life.
The present invention proposes a kind of yellow twilight sunset devitrified glass and preparation method thereof, launches gold-tinted at blue-light excited lower material; After exciting stopping, material produces bright gold-tinted twilight sunset and launches.Under alternating-current drives, the stroboscopic effect of the AC-LED device built based on this devitrified glass obtains significantly to be improved, and the stroboscopic degree of depth is only 49.5%.
Summary of the invention
The present invention relates to a class containing Ln 3al 2ga 3o 12: Ce, R are (a kind of in Ln=Y, Gd, Lu; R=Cr, a kind of in Bi) devitrified glass of crystalline phase and technology of preparing thereof, object is to prepare that physical and chemical performance is stable, yellow twilight sunset efficiently can be excited by blue light, afterglow intensity is high, time of persistence is controlled in the white light AC-LED fluorescent materials for lamp of millisecond magnitude (5-20 millisecond).
The present invention is achieved through the following technical solutions:
A kind of glass basis, is characterized in that: the glass ingredient content (mol%) of described glass basis is as follows:
15-35mol％SiO 2；10-30mol％Al 2O 3；10-25mol％Ln 2O 3；5-20mol％Ga 2O 3；0-15mol％B 2O 3；0-15mol％Ae 2O；0-5mol％ZrO 2；0-5mol％TiO 2；0.01-0.1mol％CeO 2；0.005-0.05mol％R 2O 3；
Wherein, Ae is selected from Li, Na or K; Ln is selected from Y, Gd or Lu; R=Cr or Bi.Mole total amount of said components is 100mol%.
A kind of Ln 3al 2ga 3o 12: Ce, R devitrified glass, is characterized in that the glass basis of described devitrified glass as previously mentioned.
Particularly, the component of described glass basis and percentage composition (mol%) as follows:
15-35mol％SiO 2；10-30mol％Al 2O 3；10-25mol％Ln 2O 3；5-20mol％Ga 2O 3；0-15mol％B 2O 3；0-15mol％Ae 2O；0-5mol％ZrO 2；0-5mol％TiO 2；0.01-0.1mol％CeO 2；0.005-0.05mol％R 2O 3。
Wherein
Ae is selected from Li, Na or K; Ln is selected from Y, Gd or Lu; R=Cr or Bi.
Mole total amount of said components is 100mol%.
According to the present invention, the preferred content of each component is as follows:
SiO 2be preferably 18-33mol%, more preferably 20-30mol%, also more preferably 24-26mol%;
Al 2o 3be preferably 12-26mol%, more preferably 15-24mol%; , also more preferably 18-22mol%;
Ln 2o 3be preferably 12-20mol%, more preferably 14-16mol%;
Ga 2o 3be preferably 8-18mol%, more preferably 12-16mol%;
B 2o 3be preferably 5-14mol%, more preferably 8-12mol%;
Ae 2o is preferably 5-13mol%, is more preferably 8-12mol%;
ZrO 2be preferably 2-3mol%;
TiO 2be preferably 2-3mol%;
CeO 2be preferably 0.04mol%;
R 2o 3be preferably 0.01mol%.
The present invention also provides a kind of Ln that can realize Millisecond gold-tinted twilight sunset and launch after blue-light excited stopping 3al 2ga 3o 12: Ce, R devitrified glass, the glass basis of described devitrified glass is as previously mentioned.
Particularly, the glass basis component of described devitrified glass and percentage composition (mol%) as follows:
15-35mol％SiO 2；10-30mol％Al 2O 3；10-25mol％Ln 2O 3；5-20mol％Ga 2O 3；0-15mol％B 2O 3；0-15mol％Ae 2O；0-5mol％ZrO 2；0-5mol％TiO 2；0.01-0.1mol％CeO 2；0.005-0.05mol％R 2O 3。
Wherein
Ae is selected from Li, Na or K; Ln is selected from Y, Gd or Lu; R=Cr or Bi.
Mole total amount of said components is 100mol%.
According to the present invention, the preferred content of each component is as follows:
SiO 2be preferably 18-33mol%, more preferably 20-30mol%, also more preferably 24-26mol%;
Al 2o 3be preferably 12-26mol%, more preferably 15-24mol%; , also more preferably 18-22mol%;
Ln 2o 3be preferably 12-20mol%, more preferably 14-16mol%;
Ga 2o 3be preferably 8-18mol%, more preferably 12-16mol%;
B 2o 3be preferably 5-14mol%, more preferably 8-12mol%;
Ae 2o is preferably 5-13mol%, is more preferably 8-12mol%;
ZrO 2be preferably 2-3mol%;
TiO 2be preferably 2-3mol%;
CeO 2be preferably 0.04mol%;
R 2o 3be preferably 0.01mol%.
Ln of the present invention 3al 2ga 3o 12: Ce, R devitrified glass, is characterized in that: micro-structural feature is Ln 3al 2ga 3o 12: Ce, R fluorescent microcrystalline is evenly embedded in oxide glass matrix.
The present invention also provides a kind of Ln 3al 2ga 3o 12: the preparation method of Ce, R devitrified glass, is characterized in that: adopt melt supercooled method in conjunction with subsequent heat treatment technique.
According to the present invention, described preparation method comprises:
(1) by SiO 2, Al 2o 3, Ln 2o 3, Ga 2o 3, B 2o 3, Ae 2o, ZrO 2, TiO 2, CeO 2and R 2o 3powder raw material weighs according to certain component proportion, put into resistance furnace and heat and be incubated and make it melting, after annealing, obtains block forerunner's glass through melt supercooled;
(2) forerunner's glass that step (1) obtains is put into resistance furnace to heat, carry out Isothermal treatment, make it generating portion crystallization, obtain block devitrified glass.
According to the present invention, in step (1), before putting into resistance furnace, first powder raw material is mixed and grind and be evenly placed in crucible.
According to the present invention, in step (1), in resistance furnace, be heated to 1400-1600 DEG C.Insulation 1-5 hour, preferred 2-4 hour makes powder raw material melting.
According to the present invention, in step (1), glass melt taking-up is also poured in mould fast and is shaped, obtain block forerunner's glass.
According to the present invention, in step (1), forerunner's glass is put into resistance furnace and anneals to eliminate internal stress.Annealing temperature is 600-850 DEG C, preferred 700-800 DEG C.Annealing time is 1-5 hour, preferred 2-4 hour.
According to the present invention, in step (2), forerunner's glass is heated to 900-1100 DEG C in resistance furnace.Insulation 1-5 hour, preferred 2-4 hour, make glass generating portion crystallization.
According to the present invention, described melt supercooled method and subsequent heat treatment technique specifically comprise the steps:
(1) by SiO 2, Al 2o 3, Ln 2o 3, Ga 2o 3, B 2o 3, Ae 2o, ZrO 2, TiO 2, CeO 2and R 2o 3powder raw material weighs according to certain component proportion, mixing in agate jar and grinding evenly is placed in crucible, put into resistance furnace be heated to 1400-1600 DEG C after insulation within 2 hours, make it melting, then, glass melt is taken out and pours in mould fast and is shaped, and put into resistance furnace in 750 DEG C of annealing 2 hours to eliminate internal stress, thus obtain block forerunner's glass;
(2) forerunner's glass of acquisition is put into after resistance furnace is heated to 900-1100 DEG C, carry out 2 hours Isothermal treatment, make it generating portion crystallization, obtain block devitrified glass.
According to the present invention, the crucible used in preparation process can be platinum crucible or corundum crucible.
In the present invention, adopt above material component and preparation technology, can obtain and evenly inlay Ln in oxide glass matrix 3al 2ga 3o 12: the transparent glass-ceramics of Ce, R crystal grain.Wherein, Ce ion is Yellow luminous center; Ga is not only defect center, and give material afterglow characteristic, also controllable matrix energy band structure, makes the twilight sunset of material efficiently can be excited by blue light; R ion works the degree of depth and the concentration that regulate defect.Transparent glass-ceramics, under 460 nano blue lights excite, sends strong gold-tinted; After blue-light excited stopping, producing bright gold-tinted twilight sunset and launch, the twilight sunset life-span is 5-20 millisecond.
The invention still further relates to a kind of application of devitrified glass, it is characterized in that, described devitrified glass is used as fluorescent material.
According to the present invention, the white light AC-LED that described devitrified glass excites for building blue chip.During energising, the white light of device emitting bright; During power-off, the afterglow of material Millisecond can make up stroboscopic.
Devitrified glass preparation technology of the present invention is simple, with low cost, and nontoxic pollution-free has good calorifics and chemical stability, is expected the high-power white light AC-LED device that Application and Development excites in structure blue chip.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of example 1 medium afterglow devitrified glass sample;
Fig. 2 is the stereoscan photograph of example 1 medium afterglow devitrified glass sample;
Fig. 3 is the exciting of example 1 medium afterglow devitrified glass sample, emmission spectrum;
Fig. 4 is the decay of afterglow curve of example 1 medium afterglow devitrified glass sample;
Fig. 5 is the internal quantum efficiency test curve of devitrified glass sample in example 1;
Fig. 6 be in example 1 devitrified glass at blue-light excited lower and luminous photo after exciting stopping;
Fig. 7 is the stroboscopic test curve of devitrified glass AC-LED device in example 1.
Embodiment
Example 1: by analytically pure SiO 2, Al 2o 3, Gd 2o 3, Ga 2o 3, B 2o 3, Na 2cO 3, ZrO 2, TiO 2, CeO 2and Bi 2o 3powder, by 15SiO 2: 20Al 2o 3: 14.98Gd 2o 3: 14.99Ga 2o 3: 10B 2o 3: 10Na 2cO 3: 2.5ZrO 2: 2.5TiO 2: 0.04CeO 2: 0.01Bi 2o 3the proportioning accurate weighing of (mol ratio) is placed in agate jar, mixing and grinding evenly is placed in platinum crucible, put into resistance furnace be heated to 1500 DEG C after insulation within 2 hours, make it melting, then, glass melt is taken out and pours in mould fast and is shaped, then put into resistance furnace and anneal 2 hours to eliminate internal stress in 750 DEG C, thus obtain block forerunner's glass.Forerunner's glass of acquisition is put into after resistance furnace is heated to 1000 DEG C, carry out 2 hours Isothermal treatment, make it generating portion crystallization, obtain containing Gd 3al 2ga 3o 12: the block devitrified glass of Ce, Bi crystalline phase.
X ray diffracting data shows in glass basis, separated out Gd 3al 2ga 3o 12: Ce, Bi micron crystalline phase (as shown in Figure 1).Scanning electron microscope result shows Gd 3al 2ga 3o 12: Ce, Bi micron crystalline substance is evenly distributed in (as shown in Figure 2) among glass basis.Sample, through surface finish, is measured its room temperature by FLS920 fluorescence spectrophotometer and is excited and emission spectrum (as shown in Figure 3).At monitoring Ce 3+in the excitation spectrum of ion 550 nanometer emission, detect corresponding to Ce 3+: the excitation band of the blue wave band (400-500 nanometer) of 4f → 5d transition; On the emission spectrum that 460 nanometers excite, occur corresponding to Ce 3+: the strong yellow emission (centre wavelength is 550 nanometers) of 5d → 4f transition; The luminous quantum efficiency of devitrified glass sample was 89.4% (as shown in Figure 4).From decay of afterglow curve (as shown in Figure 5), the twilight sunset life-span of devitrified glass sample is Millisecond (being about 14.5 milliseconds).Under 460 nano blue lights excite, electromagnetic radiation gold-tinted, gold-tinted and blue light combine and produce bright white light; After exciting stopping, sample produces gold-tinted twilight sunset and launches (as shown in Figure 6).Under alternating-current drives, test the stroboscopic curve (as shown in Figure 7) of the AC-LED device built based on this devitrified glass, as calculated, the stroboscopic degree of depth is 49.5%.
Example 2: by analytically pure SiO 2, Al 2o 3, Y 2o 3, Ga 2o 3, B 2o 3, K 2cO 3, ZrO 2, CeO 2and Cr 2o 3powder, by 20SiO 2: 25Al 2o 3: 11.99Y 2o 3: 18.99Ga 2o 3: 5B 2o 3: 15K 2cO 3: 5ZrO 2: 0.02CeO 2: 0.01Cr 2o 3the proportioning accurate weighing of (mol ratio) is placed in agate jar, mixing and grinding evenly is placed in platinum crucible, put into resistance furnace be heated to 1600 DEG C after insulation within 3 hours, make it melting, then, glass melt is taken out and pours in mould fast and is shaped, then put into resistance furnace and anneal 2 hours to eliminate internal stress in 800 DEG C, thus obtain block forerunner's glass.Forerunner's glass of acquisition is put into after resistance furnace is heated to 1100 DEG C, carry out 4 hours Isothermal treatment, make it generating portion crystallization, obtain containing Y 3al 2ga 3o 12: the block devitrified glass of Ce, Cr crystalline phase.Under 460 nano blue lights excite, electromagnetic radiation gold-tinted, gold-tinted and blue light combine and produce bright white light; After exciting stopping, sample produces gold-tinted twilight sunset and launches.Under alternating-current drives, the stroboscopic degree of depth of the AC-LED device built based on this devitrified glass is 55.3%.
Example 3: by analytically pure SiO 2, Al 2o 3, Lu 2o 3, Ga 2o 3, B 2o 3, Li 2cO 3, TiO 2, CeO 2and Cr 2o 3powder, by 15SiO 2: 30Al 2o 3: 19.99Lu 2o 3: 9.99Ga 2o 3: 12B 2o 3: 8Li 2cO 3: 5TiO 2: 0.02CeO 2: 0.01Cr 2o 3the proportioning accurate weighing of (mol ratio) is placed in agate jar, mixing and grinding evenly is placed in platinum crucible, put into resistance furnace be heated to 1400 DEG C after insulation within 5 hours, make it melting, then, glass melt is taken out and pours in mould fast and is shaped, then put into resistance furnace and anneal 3 hours to eliminate internal stress in 650 DEG C, thus obtain block forerunner's glass.Forerunner's glass of acquisition is put into after resistance furnace is heated to 900 DEG C, carry out 3 hours Isothermal treatment, make it generating portion crystallization, obtain containing Lu 3al 2ga 3o 12: the block devitrified glass of Ce, Cr crystalline phase.Under 460 nano blue lights excite, electromagnetic radiation gold-tinted, gold-tinted and blue light combine and produce bright white light; After exciting stopping, sample produces gold-tinted twilight sunset and launches.Under alternating-current drives, the stroboscopic degree of depth of the AC-LED device built based on this devitrified glass is 64.6%.
Example 4: by analytically pure SiO 2, Al 2o 3, Gd 2o 3, Ga 2o 3, Li 2cO 3, TiO 2, ZrO 2, CeO 2and Cr 2o 3powder, by 30SiO 2: 15Al 2o 3: 17.98Gd 2o 3: 11.995Ga 2o 3: 15Li 2cO 3: 5TiO 2: 5ZrO 2: 0.04CeO 2: 0.005Cr 2o 3the proportioning accurate weighing of (mol ratio) is placed in agate jar, mixing and grinding evenly is placed in platinum crucible, put into resistance furnace be heated to 1550 DEG C after insulation within 4 hours, make it melting, then, glass melt is taken out and pours in mould fast and is shaped, then put into resistance furnace and anneal 3 hours to eliminate internal stress in 850 DEG C, thus obtain block forerunner's glass.Forerunner's glass of acquisition is put into after resistance furnace is heated to 1100 DEG C, carry out 4 hours Isothermal treatment, make it generating portion crystallization, obtain containing Gd 3al 2ga 3o 12: the block devitrified glass of Ce, Cr crystalline phase.Under 460 nano blue lights excite, electromagnetic radiation gold-tinted, gold-tinted and blue light combine and produce bright white light; After exciting stopping, sample produces gold-tinted twilight sunset and launches.Under alternating-current drives, the stroboscopic degree of depth of the AC-LED device built based on this devitrified glass is 58.4%.
Example 5: by analytically pure SiO 2, Al 2o 3, Y 2o 3, Ga 2o 3, B 2o 3, TiO 2, ZrO 2, CeO 2and Bi 2o 3powder, by 28SiO 2: 17Al 2o 3: 15.98Y 2o 3: 13.995Ga 2o 3: 15B 2o 3: 5TiO 2: 5ZrO 2: 0.04CeO 2: 0.005Bi 2o 3the proportioning accurate weighing of (mol ratio) is placed in agate jar, mixing and grinding evenly is placed in platinum crucible, put into resistance furnace be heated to 1450 DEG C after insulation within 5 hours, make it melting, then, glass melt is taken out and pours in mould fast and is shaped, then put into resistance furnace and anneal 3 hours to eliminate internal stress in 850 DEG C, thus obtain block forerunner's glass.Forerunner's glass of acquisition is put into after resistance furnace is heated to 1100 DEG C, carry out 5 hours Isothermal treatment, make it generating portion crystallization, obtain containing Y 3al 2ga 3o 12: the block devitrified glass of Ce, Cr crystalline phase.Under 460 nano blue lights excite, electromagnetic radiation gold-tinted, gold-tinted and blue light combine and produce bright white light; After exciting stopping, sample produces gold-tinted twilight sunset and launches.Under alternating-current drives, the stroboscopic degree of depth of the AC-LED device built based on this devitrified glass is 69%.
Example 6: by analytically pure SiO 2, Al 2o 3, Lu 2o 3, Ga 2o 3, B 2o 3, ZrO 2, CeO 2and Bi 2o 3powder, by 35SiO 2: 10Al 2o 3: 24.995Lu 2o 3: 4.99Ga 2o 3: 10B 2o 3: 10K 2cO 3: 5ZrO 2: 0.01CeO 2: 0.01Cr 2o 3the proportioning accurate weighing of (mol ratio) is placed in agate jar, mixing and grinding evenly is placed in platinum crucible, put into resistance furnace be heated to 1500 DEG C after insulation within 4 hours, make it melting, then, glass melt is taken out and pours in mould fast and is shaped, then put into resistance furnace and anneal 2 hours to eliminate internal stress in 800 DEG C, thus obtain block forerunner's glass.Forerunner's glass of acquisition is put into after resistance furnace is heated to 1000 DEG C, carry out 3 hours Isothermal treatment, make it generating portion crystallization, obtain containing Lu 3al 2ga 3o 12: the block devitrified glass of Ce, Bi crystalline phase.Under 460 nano blue lights excite, electromagnetic radiation gold-tinted, gold-tinted and blue light combine and produce bright white light; After exciting stopping, sample produces gold-tinted twilight sunset and launches.Under alternating-current drives, the stroboscopic degree of depth of the AC-LED device built based on this devitrified glass is 72.3%.

Claims (7)

1. a glass basis, is characterized in that: the glass ingredient content (mol%) of described glass basis is as follows: 15-35mol%SiO 2; 10-30mol%Al 2o 3; 10-25mol%Ln 2o 3; 5-20mol%Ga 2o 3; 0-15mol%B 2o 3; 0-15mol%Ae 2o; 0-5mol%ZrO 2; 0-5mol%TiO 2; 0.01-0.1mol%CeO 2; 0.005-0.05mol%R 2o 3; Wherein, Ae is selected from Li, Na or K; Ln is selected from Y, Gd or Lu; R=Cr or Bi.Mole total amount of said components is 100mol%.
2. the Ln that can realize blue-light excited high efficiency yellow twilight sunset and launch 3al 2ga 3o 12: Ce, R devitrified glass, the glass basis of described devitrified glass is as claimed in claim 1.
3. Ln according to claim 2 3al 2ga 3o 12: Ce, R devitrified glass, is characterized in that, micro-structural feature is Ln 3al 2ga 3o 12: Ce, R fluorescent microcrystalline is evenly embedded in described glass basis.
4. the Ln described in a Claims 2 or 3 3al 2ga 3o 12: the preparation method of Ce, R devitrified glass, is characterized in that, described method comprises melt supercooled method in conjunction with subsequent heat treatment technique.
5. preparation method according to claim 4, is characterized in that, described in comprise:
(1) by SiO 2, Al 2o 3, Ln 2o 3, Ga 2o 3, B 2o 3, Ae 2o, ZrO 2, TiO 2, CeO 2and R 2o 3powder raw material weighs according to certain component proportion, put into resistance furnace and heat and be incubated and make it melting, after annealing, obtains block forerunner's glass through melt supercooled;
(2) forerunner's glass that step (1) obtains is put into resistance furnace to heat, carry out Isothermal treatment, make it generating portion crystallization, obtain block devitrified glass.
6. the preparation method according to claim 4 or 5, is characterized in that, described melt supercooled method specifically comprises the steps: in conjunction with thermal treatment process
(1) by SiO 2, Al 2o 3, Ln 2o 3, Ga 2o 3, B 2o 3, Ae 2o, ZrO 2, TiO 2, CeO 2and R 2o 3powder raw material weighs according to certain component proportion, mixing in agate jar and grinding evenly is placed in crucible, put into resistance furnace be heated to 1400-1600 DEG C after insulation within 2 hours, make it melting, then, glass melt is taken out and pours in mould fast and is shaped, and put into resistance furnace in 750 DEG C of annealing 2 hours to eliminate internal stress, thus obtain block forerunner's glass;
(2) forerunner's glass of acquisition is put into after resistance furnace is heated to 900-1100 DEG C, carry out 2 hours Isothermal treatment, make it generating portion crystallization, obtain block devitrified glass.
7. the Ln described in a Claims 2 or 3 3al 2ga 3o 12: the application of Ce, R devitrified glass, is characterized in that, described devitrified glass as fluorescent material, preferably, the long-range white light AC-LED of superpower that described devitrified glass excites for building blue chip.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271760A (en) * 2015-11-05 2016-01-27 中国科学院福建物质结构研究所 Glass ceramics for AC-LED and preparation method thereof
CN106746678A (en) * 2016-12-02 2017-05-31 中国科学院福建物质结构研究所 A kind of short persistence glass ceramics for exchanging white light LEDs
CN108483926A (en) * 2018-03-16 2018-09-04 华南理工大学 One kind is from crystallization devitrified glass and its preparation method and application
CN109444096A (en) * 2018-10-24 2019-03-08 中国科学院福建物质结构研究所 A kind of solid phase detection methods of lead ion
CN112851124A (en) * 2021-02-04 2021-05-28 中国科学院福建物质结构研究所 Glass ceramic membrane composite material for laser illumination
CN114380505A (en) * 2022-02-25 2022-04-22 中国计量大学 Sunlight-excited ultra-long afterglow microcrystalline glass and preparation method thereof

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CN105271760A (en) * 2015-11-05 2016-01-27 中国科学院福建物质结构研究所 Glass ceramics for AC-LED and preparation method thereof
CN105271760B (en) * 2015-11-05 2019-03-08 中国科学院福建物质结构研究所 A kind of AC-LED devitrified glass and preparation method thereof
CN106746678A (en) * 2016-12-02 2017-05-31 中国科学院福建物质结构研究所 A kind of short persistence glass ceramics for exchanging white light LEDs
CN108483926A (en) * 2018-03-16 2018-09-04 华南理工大学 One kind is from crystallization devitrified glass and its preparation method and application
CN108483926B (en) * 2018-03-16 2020-11-24 华南理工大学 Self-crystallization microcrystalline glass and preparation method and application thereof
CN109444096A (en) * 2018-10-24 2019-03-08 中国科学院福建物质结构研究所 A kind of solid phase detection methods of lead ion
CN109444096B (en) * 2018-10-24 2021-07-16 中国科学院福建物质结构研究所 Solid-phase detection method for lead ions
CN112851124A (en) * 2021-02-04 2021-05-28 中国科学院福建物质结构研究所 Glass ceramic membrane composite material for laser illumination
CN114380505A (en) * 2022-02-25 2022-04-22 中国计量大学 Sunlight-excited ultra-long afterglow microcrystalline glass and preparation method thereof
CN114380505B (en) * 2022-02-25 2023-03-07 中国计量大学 Sunlight-excited ultra-long afterglow microcrystalline glass and preparation method thereof

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